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Method for producing medical raw material DM by using oxydol as oxidant

A technology of hydrogen peroxide and oxidant, applied in the direction of organic chemistry, etc., can solve the problems of low purity of DM, adverse effects of surrounding environment, inability to

Inactive Publication Date: 2010-12-01
KEMAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Generally, the purity of DM synthesized by existing methods is not high, and its melting point is generally around 170-172°C. It can only be used as a rubber vulcanization accelerator, and cannot be used as a raw material for synthetic medicine. It is necessary to further purify DM or improve the synthesis process of DM.
The literature (Polymer and Auxiliary, 2004, 2:38) reported the refining of industrial DM with benzene solvents, and the method of preparing DM. The melting point of the obtained DM can reach 181°C, which basically meets the requirements for the manufacture of active esters. However, the use of benzene solvents will have adverse effects on both the operator and the surrounding environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0008] The weight ratio of water and rubber accelerator M is 1:1, add it into the reaction kettle, add sodium hydroxide with a molar ratio of rubber accelerator M of 1:1, and add the M sodium salt liquid formed by the reaction into the oxidation kettle, and then add The volume ratio with M sodium salt liquid is the solvent (solvent is water) of 1: 1, under the reaction temperature of 40 DEG C, in solution, drip the mixed oxidant solution that sulfuric acid and hydrogen peroxide weight ratio are 1: 2, flow velocity is 50ml / Minutes, until the pH of the solution is 8, stop adding the mixed oxidant, suction filter, wash with water, filter, and dry to obtain the pharmaceutical raw material DM product, and the yield of the pharmaceutical raw material DM reaches more than 94%. The invention has the advantages that the sodium sulfate in the water can be recovered, and the water and isopropanol can be recycled, which conforms to the national environmental protection policy. The purity...

example 2

[0010] The weight ratio of water and rubber accelerator M is 1:1, add it into the reactor, add sodium hydroxide with a molar ratio of rubber accelerator M of 1:1.5, and add the M sodium salt liquid formed by the reaction into the oxidation kettle, and then add The volume ratio of the M sodium salt liquid is 1:2 solvent (the solvent is ethanol), at a reaction temperature of 40°C, add dropwise a mixed oxidant solution with a weight ratio of sulfuric acid and hydrogen peroxide of 1:2 to the solution, and the flow rate is 50 per minute, until the pH of the solution is 8, stop adding the mixed oxidizing agent dropwise, filter with suction, wash with water, filter, and dry to obtain the pharmaceutical raw material DM product, and the yield of the pharmaceutical raw material DM reaches more than 95%. The invention has the advantages that the sodium sulfate in the water can be recovered, and the water and isopropanol can be recycled, which conforms to the national environmental protect...

example 3

[0012] The weight ratio of water and rubber accelerator M is 11, and put into the reaction kettle, add sodium hydroxide with a molar ratio of 1:1.2 to the rubber accelerator M, and add the M sodium salt liquid generated by the reaction into the oxidation kettle, and then add the mixture with M The volume ratio of the sodium salt liquid is a solvent (the solvent is acetone) of 1:3, and at a reaction temperature of 40°C, add dropwise a mixed oxidant solution with a weight ratio of sulfuric acid and hydrogen peroxide of 1:3 to the solution, and the flow rate is 50 / min Yes, until the pH of the solution is 4, stop adding the mixed oxidizing agent dropwise, filter with suction, wash with water, filter, and dry to obtain the pharmaceutical raw material DM product, and the yield of the pharmaceutical raw material DM reaches more than 95%. The invention has the advantages that the sodium sulfate in the water can be recovered, and the water and isopropanol can be recycled, which conforms...

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Abstract

The invention discloses a method for producing a medical raw material DM by using oxydol as an oxidant, which comprises the following steps of: adding water and a rubber accelerator M into a reaction kettle in a weight ratio of 1-15:1; adding sodium hydroxide into the reaction kettle in a molar ratio of 1:1-3 with the rubber accelerator M; adding M sodium salt liquid generated after reaction into an oxidation kettle, and adding a solvent (water, ethanol, methanol, isopropyl alcohol, acetone, aniline, toluene and the like) into the oxidation kettle in a volume ratio of 1:1-10 with the M sodium salt liquid; under the condition that the temperature is between 40 and 70 DEG C, dropping mixed oxidant solution of which the weight ratio of sulfuric acid to the oxydol is 1:1-12 into the mixture at a flow rate of 50 to 110 ml / minute, and stopping dropping the mixed oxidant when the pH of the solution is 4 to 8; and performing suction filtration, water washing, filtration and drying to obtain a product of the medical raw material DM, wherein the yield of the medical raw material DM is over 95 percent. The method has the following advantages that: sodium sulfate in the water can be reclaimed; the water and the isopropyl alcohol can be recycled; the method accords with a national environmental protection policy; and the purity of the medical raw material DM can reach 99 percent, and the melting point can be over 178 DEG C.

Description

technical field [0001] The invention relates to a production method of benzothiazole disulfide (DM), a medical raw material, and belongs to the technical field of DM production of medical raw materials. Background technique [0002] Pharmaceutical raw material DM is an intermediate for the production of third-generation cephalosporin antibiotics trixone and thioxime. Generally, the purity of DM synthesized by existing methods is not high, and its melting point is generally around 170-172°C. It can only be used as a rubber vulcanization accelerator, and cannot be used as a raw material for synthetic medicine. It is necessary to further purify DM or improve the synthesis process of DM. . The literature (Polymer and Auxiliary, 2004, 2:38) reported the refining of industrial DM with benzene solvents, and the method of preparing DM. The melting point of the obtained DM can reach 181°C, which basically meets the requirements for the manufacture of active esters. However, the use...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/78
Inventor 朱军薛兴杰
Owner KEMAI CHEM
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